公开(公告)号：US08981079B2

公开(公告)日：2015-03-17

申请号：US13378531

申请日：2010-06-18

Applicant: James Edwin Wiley, Jr. ,  Mohamad R. Jaber

Inventor： James Edwin Wiley, Jr. ,  Mohamad R. Jaber

IPC: C07H5/02 ,  C07C233/03 ,  C07C231/24 ,  C07H1/06

CPC classification number: C07C231/24 ,  C07H1/06 ,  C07H5/02 ,  C07C233/03

Abstract: A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).

Abstract translation: 使用氯化剂如氯亚胺鎓物质来除去或中和作为叔甲酰胺溶剂中的污染物存在的叔乙酰胺。 以这种方式纯化或处理的叔甲酰胺溶剂可用作蔗糖-6-酰化物氯化反应载体，从而提高所需三氯半乳蔗糖-6-酰化物（三氯蔗糖生产中的中间体）的产率。

公开(公告)号：US20120289693A1

公开(公告)日：2012-11-15

申请号：US13463332

申请日：2012-05-03

Applicant: David T. Coleman ,  Edward Micinski ,  James Edwin Wiley, JR. ,  Thomas A. Eilers ,  David A. Dentel

Inventor： David T. Coleman ,  Edward Micinski ,  James Edwin Wiley, JR. ,  Thomas A. Eilers ,  David A. Dentel

IPC: C07C231/24 ,  C07H1/06 ,  C07H1/00

CPC classification number: B01D11/04 ,  C07H13/02

Abstract: A method of removing a carboxylic acid from a liquid including a tertiary amide solvent includes: A) forming an extraction medium including an acid-extracting tin species and an extraction solvent that is immiscible with the tertiary amide solvent; B) subsequently contacting the liquid with the extraction medium, forming a phase including a de-acidified tertiary amide solvent and a phase including the extraction solvent; and C) removing the phase including the extraction solvent, to afford a liquid including the de-acidified tertiary amide solvent. The acid-extracting tin species is one or more tin species obtainable by reaction of a di(hydrocarbyl)tin oxide with less than one equivalent of a carboxylic acid, tin species obtainable by reaction of a 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxane with an aqueous base. A method of preparing a sucralose-6-acylate includes using the foregoing method to remove a carboxylic acid from a liquid including a tertiary amide solvent and the sucralose-6-acylate.

Abstract translation: 从包括叔酰胺溶剂的液体中除去羧酸的方法包括：A）形成包含酸提取锡物质的萃取介质和与叔酰胺溶剂不混溶的萃取溶剂; B）随后使液体与提取介质接触，形成包含脱酸叔胺溶剂和包含萃取溶剂的相的相; 和C）除去包括萃取溶剂的相，得到包含脱酸叔酰胺溶剂的液体。 酸提取锡物质是通过二（烃基）氧化锡与小于1当量羧酸反应获得的一种或多种锡物质，可通过1,3-二酰氧基-1,1， 3,3-四（烃基）二锡氧烷与碱水溶液。 制备三氯蔗糖-6-酰化物的方法包括使用上述方法从包括叔酰胺溶剂和三氯蔗糖-6-酰化物的液体中除去羧酸。

公开(公告)号：US08212022B2

公开(公告)日：2012-07-03

申请号：US12416520

申请日：2009-04-01

Applicant: Edward Micinski ,  James Edwin Wiley, Jr.

Inventor： Edward Micinski ,  James Edwin Wiley, Jr.

IPC: C07H1/06

CPC classification number: C07H1/06 ,  C07H5/02

Abstract: A process for the purification of aqueous feed streams containing sucralose and/or sucralose 6-esters includes, providing an aqueous feed stream including the sucralose and/or sucralose 6-esters, concentrating the aqueous feed stream to form a concentrated aqueous feed stream containing at least 10 wt % total carbohydrates and extracting the concentrated aqueous feed stream with an organic solvent and producing an organic extract and an aqueous extract, in which the organic solvent is immiscible with water, and in which the carbohydrate preferentially passes into the organic extract.

Abstract translation: 用于纯化含有三氯蔗糖和/或三氯蔗糖-6-酯的含水进料流的方法包括提供包含三氯半乳蔗糖和/或三氯蔗糖6-酯的含水进料流，浓缩含水进料流以形成含有 至少10重量％的总碳水化合物，并用有机溶剂萃取浓缩的含水进料流，并产生有机萃取物和水提取物，其中有机溶剂与水不混溶，并且其中碳水化合物优先进入有机萃取物。

公开(公告)号：US20120157675A1

公开(公告)日：2012-06-21

申请号：US13378531

申请日：2010-06-18

Applicant: James Edwin Wiley, JR. ,  Mohamad R. Jaber

Inventor： James Edwin Wiley, JR. ,  Mohamad R. Jaber

IPC: C07H5/02 ,  C07C233/03

CPC classification number: C07C231/24 ,  C07H1/06 ,  C07H5/02 ,  C07C233/03

Abstract: A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).

Abstract translation: 使用氯化剂如氯亚胺鎓物质来除去或中和作为叔甲酰胺溶剂中的污染物存在的叔乙酰胺。 以这种方式纯化或处理的叔甲酰胺溶剂可用作蔗糖-6-酰化物氯化反应载体，从而提高所需三氯半乳蔗糖-6-酰化物（三氯蔗糖生产中的中间体）的产率。

公开(公告)号：US20110294083A1

公开(公告)日：2011-12-01

申请号：US13142555

申请日：2009-12-29

Applicant: James Edwin Wiley ,  William Akers ,  William R. Skelding

Inventor： James Edwin Wiley ,  William Akers ,  William R. Skelding

IPC: F24J3/00 ,  B01J19/00

CPC classification number: B01J10/005 ,  A62D3/32 ,  A62D2101/22 ,  A62D2203/10 ,  B01D47/00 ,  B01J4/008 ,  B01J2219/00182 ,  B01J2219/00247

Abstract: A molten salt treatment system and process can include one or more tubular conduits flowably connected to a molten salt reactor, the tubular conduit containing concentrically within it a pipe or a shaft separated by an annular space therebetween, and one or more gas sources connected to feed gas into the annular space. The system may include a scrubbing device flowably connected to a molten salt reactor off-gas outlet to receive an off-gas, a first heating device configured to heat the effluent from the scrubbing device, and a filtering device flowably connected to receive the effluent from the heating device. An overflow conduit may be flowably connected to a molten salt reactor overflow outlet to receive molten salt therefrom and discharge the molten salt to a salt recovery vessel, and a blower or other gas mover may be connected to the molten salt reactor and the recovery vessel to prevent backflow of cold gases through the overflow outlet to the molten salt reactor.

Abstract translation: 熔盐处理系统和过程可以包括一个或多个可流动地连接到熔盐反应器的管状导管，管状导管同心地包含一个管或由它们之间的环形空间隔开的轴，以及连接到进料的一个或多个气源 气体进入环形空间。 该系统可以包括可流动地连接到熔盐反应器废气出口以接收废气的洗涤装置，被配置为加热来自洗涤装置的流出物的第一加热装置和可流动地连接以接收来自 加热装置。 溢流导管可以可流动地连接到熔盐反应器溢流出口，以从其中接收熔融盐，并将熔融盐排出到盐回收容器中，并且鼓风机或其它气体移动器可以连接到熔盐反应器和回收容器 防止冷气体通过溢流出口回流到熔盐反应器。

公开(公告)号：US20110087018A1

公开(公告)日：2011-04-14

申请号：US12901808

申请日：2010-10-11

Applicant: Edward Micinski ,  David Coleman ,  James Edwin Wiley, JR.

Inventor： Edward Micinski ,  David Coleman ,  James Edwin Wiley, JR.

IPC: C07H1/00

CPC classification number: C07H13/04 ,  C07F7/2224 ,  C07H13/06 ,  C07H13/08

Abstract: A method for the preparation of a sucrose-6-ester is disclosed. In a first step of the method, sucrose in a polar aprotic solvent is reacted with an organotin-based acylation promoter. The water of reaction is removed at a temperature that does not exceed about 80° C. In one aspect, the water is removed by distillation of part of the polar aprotic solvent at reduced pressure. In a second step, a carboxylic acid anhydride is added. In one aspect, the resulting reaction mixture is maintained at a temperature of 10° C. or less for a period of time sufficient to produce a sucrose-6-ester. The sucrose-6-ester can be converted to sucralose.

Abstract translation: 公开了制备蔗糖-6-酯的方法。 在该方法的第一步中，将极性非质子溶剂中的蔗糖与基于有机锡的酰化促进剂反应。 在不超过约80℃的温度下除去反应水。在一个方面，通过在减压下蒸馏部分极性非质子溶剂除去水。 在第二步中，加入羧酸酐。 一方面，所得反应混合物在10℃或更低的温度下保持足以产生蔗糖-6-酯的时间。 蔗糖-6-酯可以转化成三氯蔗糖。

公开(公告)号：US20100081803A1

公开(公告)日：2010-04-01

申请号：US12416520

申请日：2009-04-01

Applicant: Edward Micinski ,  James Edwin Wiley, JR.

Inventor： Edward Micinski ,  James Edwin Wiley, JR.

IPC: C07H1/06

CPC classification number: C07H1/06 ,  C07H5/02

Abstract: A process for the purification of aqueous feed streams containing sucralose comprises: a) extracting an aqueous feed stream comprising sucralose with a first organic solvent and producing a first organic extract and a first aqueous extract, in which the organic solvent is immiscible with water, and a portion of the sucralose passes into the first organic extract; b) optionally extracting the first organic extract with an aqueous solvent to produce a second organic extract and a second aqueous extract, in which the sucralose preferentially passes into the second aqueous extract, and in which the second aqueous extract is recycled to step a); c) concentrating the first aqueous extract to form a concentrated aqueous feed stream; and d) extracting the concentrated aqueous feed stream with a second organic solvent and producing a third organic extract and a third aqueous extract, in which the second organic solvent is immiscible with water, and in which the sucralose preferentially passes into the third organic extract. A process for the purification of aqueous feed streams containing sucralose-6-esters comprises the steps of: a) providing an aqueous feed stream comprising a carbohydrate selected from the group consisting of sucralose 6-esters, and mixtures thereof with sucralose; b) concentrating the aqueous feed stream to form a concentrated aqueous feed stream; and c) extracting the concentrated aqueous feed stream with an organic solvent and producing an organic extract and an aqueous extract, in which the organic solvent is immiscible with water, and in which the carbohydrate preferentially passes into the organic extract.

Abstract translation: 用于纯化含有三氯蔗糖的含水进料流的方法包括：a）用第一有机溶剂萃取包含三氯蔗糖的含水进料流，并产生第一有机萃取物和第一含水萃取物，其中有机溶剂与水不混溶，以及 一部分三氯蔗糖进入第一有机提取物; b）任选地用水性溶剂萃取第一有机提取物以产生第二有机提取物和第二含水提取物，其中三氯蔗糖优先进入第二水提取物，并且其中第二水提取物再循环至步骤a）; c）浓缩第一含水提取物以形成浓缩的含水进料流; 和d）用第二有机溶剂萃取浓缩的含水进料流，并产生第三有机萃取物和第三含水萃取物，其中第二有机溶剂与水不混溶，其中三氯蔗糖优先进入第三有机萃取物。 用于纯化含有三氯蔗糖-6-酯的含水进料流的方法包括以下步骤：a）提供含有选自三氯蔗糖-6-酯及其与三氯半乳蔗糖的混合物的碳水化合物的含水进料流; b）浓缩含水进料流以形成浓缩的含水进料流; 和c）用有机溶剂萃取浓缩的含水进料流并制备有机萃取物和水提取物，其中有机溶剂与水不混溶，并且其中碳水化合物优先进入有机萃取物。

公开(公告)号：US20090264633A1

公开(公告)日：2009-10-22

申请号：US12345998

申请日：2008-12-30

Applicant: John Kerr ,  Robert Jansen ,  Duane A. Leinhos ,  James Edwin Wiley, JR. ,  Sebastien Camborieux ,  Anthony Baiada ,  Gordon Walker ,  Carlo Maffezzoni

Inventor： John Kerr ,  Robert Jansen ,  Duane A. Leinhos ,  James Edwin Wiley, JR. ,  Sebastien Camborieux ,  Anthony Baiada ,  Gordon Walker ,  Carlo Maffezzoni

IPC: C07H15/00

CPC classification number: C07H1/06 ,  C07H5/02

Abstract: The present invention provides a method for producing sucralose from a feed stream resulting from the chlorination of a sucrose-6-acylate in a reaction vehicle. The feed stream includes a sucralose-6-acylate, the reaction vehicle, water, and salts. The salts include one or more selected from the group consisting of alkali metal chlorides, alkaline earth metal chlorides and ammonium chloride. The method includes: (i) deacylation of the sucralose-6-acylate by treatment with a base to afford a product stream comprising sucralose; (ii) partial removal of water and, optionally, reaction vehicle from the product stream of (i) in order to cause precipitation of the salts from the product stream; (iii) removal of the precipitated salts from the product stream of (ii); and (iv) isolation of sucralose from the product stream of (iii).

Abstract translation: 本发明提供了由反应载体中蔗糖-6-酰化物的氯化得到的进料流中生产三氯蔗糖的方法。 进料流包括三氯蔗糖-6-酰化物，反应载体，水和盐。 所述盐包括选自碱金属氯化物，碱土金属氯化物和氯化铵中的一种或多种。 该方法包括：（i）用碱处理三氯半乳蔗糖-6-酰化物脱酰基，得到包含三氯蔗糖的产物流; （ii）从（i）的产物流中部分除去水和任选的反应载体，以便使产物流中的盐沉淀; （iii）从（ii）的产物流中除去沉淀的盐; 和（iv）从（iii）的产物流中分离三氯半乳蔗糖。

公开(公告)号：US20080227971A1

公开(公告)日：2008-09-18

申请号：US12004260

申请日：2007-12-20

Applicant: Duane A. Leinhos ,  David A. Dentel ,  James Edwin Wiley

Inventor： Duane A. Leinhos ,  David A. Dentel ,  James Edwin Wiley

IPC: C07H1/06

CPC classification number: C07H5/02

Abstract: A method of making sucralose includes maintaining a solution of a sucralose-6-acylate in an aqueous solvent at a temperature in a range from −20° C. to 20° C. and at a pH of at least 12.2 and less than 14.0 for a period of time sufficient to deacylate substantially all of the sucralose-6-acylate. The method may employ purified sucralose-6-acylate as the starting material, or the sucralose-6-acylate may be present in a quenched reaction mixture resulting from chlorination of a sucrose-6-acylate. The quenched reaction mixture may be exposed to deacylation conditions either before or after removal of a tertiary amide that may be present in it. Sucralose is subsequently recovered to complete the process.

Abstract translation: 制备三氯蔗糖的方法包括在-20℃至20℃的温度范围内保持三氯蔗糖-6-酰化物在水性溶剂中的溶液，并且在至少12.2和小于14.0的pH下保持 足以使基本上所有的三氯蔗糖-6-酰化物脱酰基化的时间。 该方法可以使用纯化的三氯半乳蔗糖-6-酰化物作为起始原料，或三氯蔗糖-6-酰化物可存在于由蔗糖-6-酰化物氯化得到的骤冷反应混合物中。 在除去可能存在的叔酰胺之前或之后，骤冷的反应混合物可能暴露于脱酰基化条件。 随后回收三氯蔗糖以完成该过程。

公开(公告)号：US08436157B2

公开(公告)日：2013-05-07

申请号：US12409951

申请日：2009-03-24

Applicant: James Edwin Wiley, Jr. ,  Duane A. Leinhos ,  David A. Dentel ,  John Kerr

Inventor： James Edwin Wiley, Jr. ,  Duane A. Leinhos ,  David A. Dentel ,  John Kerr

IPC: C07H1/00

CPC classification number: C07H5/02 ,  C07H1/00

Abstract: The present invention provides a method for producing sucralose from a feed stream including a sucrose-6-acylate in a reaction vehicle. The method includes: (i) reacting the sucrose-6-acylate with a chlorinating agent in order to chlorinate the 4, 1′ and 6′ positions of the sucrose-6-acylate; (ii) quenching the product stream of (i) with an aqueous solution of a base to provide a sucralose-6-acylate and the chloride salt of said base, wherein the concentration of the aqueous solution of the base is sufficiently high such that at least a portion of the chloride salt of the base is formed as a precipitate; (iii) either: deacylating the sucralose-6-acylate by treating the product stream of (ii) with a base and thereafter removing precipitated salt to provide a product stream including sucralose; or: removing precipitated salt from the product stream of (ii) and thereafter deacylating the sucralose-6-acylate by treating with a base to provide a product stream including sucralose; and (iv) isolating sucralose from the product stream of (iii).

Abstract translation: 本发明提供了在反应载体中从包含蔗糖-6-酰化物的进料流中制备三氯半乳蔗糖的方法。 该方法包括：（i）使蔗糖-6-酰化物与氯化剂反应，以使蔗糖-6-酰化物的4,1'和6'位置氯化; （ii）用碱的水溶液淬灭（i）的产物流，得到三氯半乳蔗糖-6-酰化物和所述碱的氯化物盐，其中碱的水溶液的浓度足够高，使得在 至少一部分碱的氯化物盐形成沉淀物; （iii）：通过用碱处理（ii）的产物流，然后除去沉淀的盐以提供包含三氯蔗糖的产物流，使三氯蔗糖-6-酰化物脱酰化; 或者：从（ii）的产物流中除去沉淀的盐，然后用碱处理三氯半乳蔗糖-6-酰化物，以提供包含三氯蔗糖的产物流; 和（iv）从（iii）的产物流中分离三氯半乳蔗糖。